WO2009076976A1 - Plaque bipolaire et procédé de réalisation d'une plaque bipolaire - Google Patents

Plaque bipolaire et procédé de réalisation d'une plaque bipolaire Download PDF

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Publication number
WO2009076976A1
WO2009076976A1 PCT/EP2007/011020 EP2007011020W WO2009076976A1 WO 2009076976 A1 WO2009076976 A1 WO 2009076976A1 EP 2007011020 W EP2007011020 W EP 2007011020W WO 2009076976 A1 WO2009076976 A1 WO 2009076976A1
Authority
WO
WIPO (PCT)
Prior art keywords
layer
bipolar plate
protective layer
oxide
plate according
Prior art date
Application number
PCT/EP2007/011020
Other languages
German (de)
English (en)
Inventor
Thomas Kiefer
Frank Tietz
Original Assignee
Elringklinger Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Elringklinger Ag filed Critical Elringklinger Ag
Priority to EP07856758A priority Critical patent/EP2113136A1/fr
Priority to PCT/EP2007/011020 priority patent/WO2009076976A1/fr
Priority to US12/079,517 priority patent/US20090155666A1/en
Publication of WO2009076976A1 publication Critical patent/WO2009076976A1/fr

Links

Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0206—Metals or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0206—Metals or alloys
    • H01M8/0208—Alloys
    • H01M8/021—Alloys based on iron
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0202—Collectors; Separators, e.g. bipolar separators; Interconnectors
    • H01M8/0204—Non-porous and characterised by the material
    • H01M8/0223—Composites
    • H01M8/0228—Composites in the form of layered or coated products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/10—Fuel cells with solid electrolytes
    • H01M8/12—Fuel cells with solid electrolytes operating at high temperature, e.g. with stabilised ZrO2 electrolyte
    • H01M2008/1293—Fuel cells with solid oxide electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to a bipolar plate for a fuel cell unit, wherein the bipolar plate comprises a carrier layer of a metallic material and a protective layer, wherein the protective layer comprises an at least binary oxide system with at least two different types of metal cations.
  • bipolar plates also referred to as interconnectors
  • ferritic, chromium oxide-forming stainless steels are used as material for bipolar plates in high-temperature fuel cells.
  • the chromium oxide formed on the surface of the bipolar plate has a comparatively high electrical conductivity, while, for example, aluminum oxide has an electrically insulating effect.
  • chromium oxide or a double layer which consists of chromium oxide and chromium-manganese oxide, forms on the surface of the chromium-forming steel.
  • the specific conductivities of these layers are in the range from about 0.01 S / cm to about 1 S / cm at an operating temperature of the fuel cell of 800 0 C.
  • the coefficient of thermal expansion of the chromium oxide and the double layer are in the range of about 6.5- 10 "6 K " 1 to about 9.1-10 "6 K “ 1 .
  • the thermal expansion coefficients of the components adjacent to the bipolar plate are approximately 12.5-10 "6 K " 1 .
  • the later operation of the high-temperature fuel cell (in particular, the SOFC (Solid Oxide Fuel Cell)) is associated with an increase in the oxide layer thickness. Due to the relatively low specific conductivity of the oxide layer, the contact resistance increases with increasing layer thickness, which is why the fuel cell stack loses power. In addition, by increasing the layer thickness of the oxide layer with an unadjusted coefficient of thermal expansion, mechanical stresses (which may be time-dependent) are induced. These mechanical stresses can lead to the formation of cracks in the used ceramic components and thus to a failure of the stack.
  • SOFC Solid Oxide Fuel Cell
  • chromium evaporation causes poisoning of the cathode, in particular during long-term operation of the fuel cell stack, as a result of which the power of the fuel cell stack is drastically reduced.
  • suitable coating of the interconnector steel for example with MnO x , the chromium evaporation can be prevented. In this case too, however, the oxide layer of the interconnector steel grows over time.
  • the present invention has for its object to provide a bipolar plate of the type mentioned, whose protective layer prevents the formation of an oxide layer or the properties of the oxide layer formed so changed that lower mechanical stresses in the oxide layer arise.
  • the oxide layer of the interconnector material which is produced during operation of the fuel cell unit can be modified such that desired material properties (for example an adapted thermal expansion coefficient, for the resulting oxide layer good electrical conductivity and high chemical stability) can be achieved.
  • desired material properties for example an adapted thermal expansion coefficient, for the resulting oxide layer good electrical conductivity and high chemical stability
  • the coating can completely prevent the formation of an oxide layer between the interconnector material and the protective layer during operation of the fuel cell unit.
  • the modification effect of the protective layer according to the invention on the oxide layer formed during operation of the fuel cell unit may be based on the formation enthalpy of the new oxide layer containing Mn and / or Cu from the protective layer being at a lower energy level than the formation enthalpy of self-forming oxidation layers of Cr 2 O 3- layers or of Cr-Mn spinel layers.
  • the oxide layer formed in the presence of the protective layer is in a metastable state and the conversion kinetics in a thermodynamically more stable range with respect to the total life of the bipolar plate is sufficiently slow.
  • the protective layer reacts more quickly with the (still) metallic ("unoxidized") surface of the material of the carrier layer than the normal oxide layer can form on the metallic material of the carrier layer, and / or when passing through an increased joining temperature (which is higher than the operating temperature of the fuel cell unit) sets a stable modified oxide layer, which is thermodynamically preferred at the joining temperature before a chromium oxide layer and then metastable at a lowering of the temperature to the operating temperature of the fuel cell unit.
  • the oxide system of the protective layer has approximately the nominal composition Mn 2 - ⁇ Cui + x 0 4 , where 0 ⁇ x ⁇ 2.
  • the oxide system with the approximate nominal composition Mn 2 CuO 4 has proved to be particularly favorable.
  • the oxide system of the protective layer is at least biphasic.
  • one phase of the oxide system of the protective layer has approximately the composition Mn 1/5 Cui, 5 O 4 and another phase of the oxide system of the protective layer has approximately the composition CuO.
  • the bipolar plate has an oxide layer formed between the carrier layer and the protective layer during operation of the fuel cell unit.
  • the chemical composition of the oxide layer is modified by the presence of the protective layer relative to the chemical composition of an oxide layer formed on the carrier layer without the protective layer during operation of the fuel cell unit.
  • the oxide layer contains no Cr spinel.
  • the oxide layer contains no Cr-Mn spinel.
  • the oxide layer formed during operation of the fuel cell unit contains Mn cations and / or Cu cations, which may originate in particular from the protective layer.
  • the composition of the protective layer of the bipolar plate is preferably selected such that the thermal expansion coefficient ⁇ of the oxide layer formed between the carrier layer and the protective layer during operation of the fuel cell unit is at least approximately 8-10 "6 K -1 . Such a thermal expansion coefficient is particularly well adapted to the thermal expansion behavior of the other components of the bipolar plate and the fuel cell unit.
  • composition of the protective layer of the bipolar plate is preferably selected such that the specific electrical conductivity ⁇ of the oxide layer formed between the carrier layer and the protective layer during operation of the fuel cell unit is at least approximately 0.1 S / cm.
  • the material of the carrier layer of the bipolar plate comprises a steel material.
  • the material of the carrier layer comprises a chromium oxide-forming steel material.
  • the properties of the oxide layer formed during operation of the fuel cell unit can be positively influenced if the material of the carrier layer is doped with Si and / or Ti.
  • the material of the carrier layer preferably contains at most 1% by weight of Si and / or at most 1% by weight of Ti.
  • the bipolar plate according to the invention is particularly suitable for use in a high-temperature fuel cell, in particular a SOFC (solid oxide fuel cell), with an operating temperature of, for example, at least 600 ° C.
  • SOFC solid oxide fuel cell
  • the present invention further relates to a method for producing a bipolar plate for a fuel cell unit.
  • the invention has the further object to provide such a method, whereby a bipolar plate is produced, the protective layer prevents the formation of an oxide layer on the carrier layer of the bipolar plate during operation of the fuel cell unit or modifies the properties of such a spontaneously formed oxide layer so that lower mechanical Tensions in the oxide layer arise.
  • the protective layer starting material is applied wet-chemically to the carrier layer.
  • the starting material can for example be sprayed onto the carrier layer or applied by screen printing or by means of a dispenser on the carrier layer.
  • Further special embodiments of the method according to the invention are subject matter of claims 21 to 26, whose features and advantages have already been explained above in connection with the particular embodiments of the bipolar plate according to the invention.
  • the electrical conductivity of the oxide layer poorly conductive in the unmodified state is improved, resulting in an improvement in the performance of the entire fuel cell stack. Aging by increasing the oxide layer thickness can also be ruled out.
  • FIG. 1 shows a schematic section through a bipolar plate with a
  • Protective layer a carrier layer and an oxide layer formed between the protective layer and the carrier layer.
  • a carrier layer made of a ferritic chromium-forming stainless steel is provided, for example made of the stainless steel Crofer 22 APU, which has the following composition: 22.2 percent by weight Cr; 0.46 weight percent Mn; 0.06 wt% Ti; 0.07 weight percent La; 0.002 weight percent C; 0.02 weight percent Al; 0.03 weight percent Si; 0.004 weight percent N; 0.02 weight percent Ni; Rest iron.
  • a paste which has the following composition is applied to this carrier layer in a screen printing process: 237.43 parts by weight of a ceramic powder; 225.56 parts by weight terpeniol; 11.9 parts by weight of ethylcellulose.
  • the ceramic powder for this paste is prepared as follows: First, an amount of two different metal oxides, such as Mn 2 O 3 and CuO, is weighed so that the number ratio of the respective metal cations (eg, Mn and Cu) corresponds to the number ratio in the desired composition of the protective layer to be produced.
  • Mn 2 O 3 and CuO the number ratio of the respective metal cations
  • the weighed metal oxide powders are filled into a polyethylene bottle along with ethanol and ZrO 2 grinding balls (approximately 0.3 mm in average diameter).
  • the weight ratio of ceramic powder (metal oxide powder): ethanol: grinding balls is preferably 1: 2: 3.
  • a dispersing agent for example, the ET-85 dispersant from Dolapix
  • a dispersing agent for example, the ET-85 dispersant from Dolapix
  • the dispersant is preferably added in a proportion of 1 percent by weight to 4 percent by weight of the ceramic powder. After reaching the desired grain size of the ceramic powder, the grinding balls are removed by sieving, and the suspension is dried.
  • the paste for the screen printing method is prepared as follows:
  • this mixture is homogenized with 237.43 parts by weight of the ceramic powder prepared in the above manner on a 3-roll mill in several stages and processed into a paste.
  • the viscosity of the paste may be from about 100 dPas to about 700 dPas.
  • the paste is applied from the protective layer precursor material to the carrier layer of the bipolar plate by means of a screen printing system known per se to a person skilled in the art, with a wet layer thickness of for example approximately 10 ⁇ m to approximately 100 ⁇ m.
  • a wet spraying method may also be used to apply the ceramic powder to the carrier layer.
  • a suspension is sprayed onto the support layer, which has the following composition: 237.43 parts by weight of a ceramic powder; 4.74 parts by weight of a dispersant (for example the dispersant designated ET-85 from Dolapix); 23.74 parts by weight of a binder (for example, polyvinyl acetate, PVAC).
  • a dispersant for example the dispersant designated ET-85 from Dolapix
  • a binder for example, polyvinyl acetate, PVAC
  • the ceramic powder for the suspension is prepared as follows: First, an amount of two different metal oxides, for example Mn 2 O 3 and CuO, is weighed so that the numerical ratio of the respective metal cations (eg Mn, Cu) corresponds to the numerical ratio in the desired composition of the protective layer to be produced.
  • Mn 2 O 3 and CuO the numerical ratio of the respective metal cations
  • the weighed metal oxide powders are filled into a polyethylene bottle along with ethanol and ZrO 2 milling balls (having a mean diameter of about 0.3 mm).
  • the grinding balls are removed by sieving from the suspension.
  • dispersant for example ET-85 from Dolapix
  • binder for example polyvinyl acetate
  • the weight ratio of the materials used in the preparation of the suspension Ceramic powder: Ethanol: Grinding balls: Dispersant: Binder is preferably about 1: 2: 3: 2x0.02: 0.1.
  • the suspension obtained in this way is sprayed onto the carrier layer by a spray nozzle in a wet spraying process.
  • the diameter of the nozzle opening, with which the suspension is atomized, is approximately 0.5 mm.
  • the injection pressure with which the suspension is conveyed to the nozzle is, for example, 0.3 bar.
  • the spraying distance of the nozzle to the carrier layer (substrate) is for example 15 cm.
  • the nozzle is moved over the carrier layer at a speed of 230 mm / s.
  • the layer of protective layer precursor is cured in one to six coating cycles, i. by spraying each surface area of the carrier layer one to six times, applied to the carrier layer.
  • both the screen-printing method and the wet-spraying method can also use corresponding amounts of metals (for example Mn, Cu) and / or calcined powder (for example Mn 2 CuO 4 ).
  • the coated carrier layer is subjected to a heat treatment.
  • the carrier layer is introduced with the protective layer precursor disposed thereon in a sintering furnace and heated to a sintering temperature.
  • the sintering temperature is higher than the operating temperature (eg, about 600 ° C. to about 900 ° C.) of the fuel cell unit in which the bipolar plate is to be used.
  • the holding time at the sintering temperature should not be longer than 10 hours.
  • the carrier layer with the applied layer of the protective layer pre-material can be subjected to a heat treatment at a sintering temperature of 950 ° C. with a holding time of 10 hours.
  • the carrier layer with the protective layer pre-material can be heated to the sintering temperature at a heating rate of, for example, 3 K / min.
  • the cooling of the carrier layer with the sintered protective layer arranged thereon, which results from the heat treatment, can be carried out by natural cooling at a cooling rate of, for example, about 10 K / min.
  • an oxide layer whose chemical composition is formed at the operating temperature of the fuel cell unit (for example, about 600 0 C to about 900 0 C) between the carrier layer and the protective layer, is changed by the coating of the steel substrate with the protective layer against the chemical composition of an oxide layer formed without the presence of such a protective layer.
  • the bipolar plate of support layer 116 generally designated 114, after oxidation during operation of the fuel cell unit, the protective layer 118 of the exemplary nominal composition Mn 2 CuO 4, and an oxide layer 120 of exemplary nominal composition formed between the support layer 116 and the protective layer 118 Cr 0/7 Mn 1/3 CuO 4 is shown in Fig. 1 in a purely schematic longitudinal section.
  • the oxide layer 120 contains no Cr spinel and no Cr-Mn spinel.
  • the oxide layer 120 shows no delamination and no material depletion due to defects or pore formation.
  • the specific electrical conductivity of the oxide layer 120 formed during operation of the fuel cell unit is greater than 40 S / cm at a temperature of 800 ° C., ie significantly higher than the specific electrical conductivity of Cr 2 O 3 at the same temperature (0.03 S / cm ).
  • the thermal expansion coefficient ⁇ of the oxide layer 120 is approximately 12-10 "6 K 1 and is thus significantly higher than the thermal expansion coefficient of Cr 2 O 3 (6.5- 10 '6 K 1 ).
  • the thermal expansion coefficient ⁇ of the oxide layer 120 is thus in the range of the thermal expansion coefficient of the other components of the fuel cell unit (from about 12-10 "6 K “ 1 to about 13-10 "6 K “ 1 ).
  • the reduction of the thermal offset results in a lowering of the undesired mechanical residual stresses of the oxide layer 120 relative to an oxide layer which is formed on the surface of the carrier layer 116 during operation of the fuel cell unit without the presence of the protective layer 118.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Fuel Cell (AREA)

Abstract

Le but de l'invention est de réaliser une plaque bipolaire pour un bloc de piles à combustible, ladite plaque bipolaire comprenant une couche de support composée d'un matériau métallique et une couche de protection qui comprend un système oxyde au moins binaire possédant au moins deux différents types de cations métalliques, ladite couche de protection empêchant la formation d'une couche d'oxyde ou modifiant les propriétés de la couche d'oxyde formée, de sorte que des contraintes mécaniques plus faibles apparaissent dans la couche d'oxyde. A cet effet, un type de cations métalliques du système oxyde de la couche de protection est Mn et un autre type de cations métalliques du système oxyde de la couche de protection est Cu.
PCT/EP2007/011020 2007-12-14 2007-12-14 Plaque bipolaire et procédé de réalisation d'une plaque bipolaire WO2009076976A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP07856758A EP2113136A1 (fr) 2007-12-14 2007-12-14 Plaque bipolaire et procédé de réalisation d'une plaque bipolaire
PCT/EP2007/011020 WO2009076976A1 (fr) 2007-12-14 2007-12-14 Plaque bipolaire et procédé de réalisation d'une plaque bipolaire
US12/079,517 US20090155666A1 (en) 2007-12-14 2008-03-27 Bipolar plate and process for producing a bipolar plate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/EP2007/011020 WO2009076976A1 (fr) 2007-12-14 2007-12-14 Plaque bipolaire et procédé de réalisation d'une plaque bipolaire

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US12/079,517 Continuation US20090155666A1 (en) 2007-12-14 2008-03-27 Bipolar plate and process for producing a bipolar plate

Publications (1)

Publication Number Publication Date
WO2009076976A1 true WO2009076976A1 (fr) 2009-06-25

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PCT/EP2007/011020 WO2009076976A1 (fr) 2007-12-14 2007-12-14 Plaque bipolaire et procédé de réalisation d'une plaque bipolaire

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EP (1) EP2113136A1 (fr)
WO (1) WO2009076976A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4145572A1 (fr) * 2021-09-06 2023-03-08 Toshiba Energy Systems & Solutions Corporation Interconnecteur revêtu d'une couche de protection, empilement de cellules comprenant cet interconnecteur revêtu d'une couche de protection et système d'énergie à hydrogène le comprenant

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5044628B2 (ja) 2009-11-09 2012-10-10 日本碍子株式会社 コーティング体
WO2014031622A1 (fr) 2012-08-21 2014-02-27 Bloom Energy Corporation Systèmes et procédés de suppression d'empoisonnement au chrome dans des piles à combustible

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WO1996028855A1 (fr) 1995-03-15 1996-09-19 Ceramic Fuel Cells Limited Dispositif d'interconnexion a pile a combustible
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WO2007093148A1 (fr) * 2006-02-18 2007-08-23 Forschungszentrum Jülich GmbH Acier ferRItique resistant au fluage

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WO1996028855A1 (fr) 1995-03-15 1996-09-19 Ceramic Fuel Cells Limited Dispositif d'interconnexion a pile a combustible
DE102005015755A1 (de) * 2005-04-06 2006-10-12 Forschungszentrum Jülich GmbH Verfahren zur Herstellung einer Chromverdampfungsschutzschicht für chromoxidbildende Metallsubstrate
WO2007093148A1 (fr) * 2006-02-18 2007-08-23 Forschungszentrum Jülich GmbH Acier ferRItique resistant au fluage

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4145572A1 (fr) * 2021-09-06 2023-03-08 Toshiba Energy Systems & Solutions Corporation Interconnecteur revêtu d'une couche de protection, empilement de cellules comprenant cet interconnecteur revêtu d'une couche de protection et système d'énergie à hydrogène le comprenant

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US20090155666A1 (en) 2009-06-18
EP2113136A1 (fr) 2009-11-04

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